摘要
随着高新领域的发展,金属锰高纯化成为行业发展的必然趋势。本工作以电解锰为原料,通过自主研发的高效蒸馏炉,结合分区冷凝,采用在冷凝区设置恒温冷凝段的方式,延长主金属冷凝区长度,达到提高金属收得率的目的,并一步制备出纯度4N5以上的高纯锰。通过对电解锰真空蒸馏理论进行分析,并研究了不同蒸馏温度、时间对挥发率和恒温冷凝段温度(冷凝温度)对金属收得率的影响,同时利用电感耦合等离子体质谱仪(ICP-MS)检测不同蒸馏温度下冷凝锰中的杂质含量。研究结果表明:在选定的蒸馏温度下主金属Mn易与杂质金属分离,但温度越高分离能力越弱。随蒸馏温度的升高和保温时间的延长,挥发率均呈上升趋势。设置主金属恒温冷凝段可大幅度提升金属收得率,随冷凝温度的升高,金属收得率呈先升后降趋势。随蒸馏温度的上升,冷凝锰中Cd、K、Na、Zn的含量基本不变,Mg、Ca、Pb、Cu、Cr、Ni、Fe、Co的含量整体呈增大趋势。综合考虑,在体系压强10^(-3)~10^(-2)Pa、冷凝温度1100℃、保温时间90 min、蒸馏温度1400℃条件下,可得纯度4N5的高纯锰,此时挥发率为86.94%,收得率可达94.32%。
With the development of high-tech fields,high purification of metal manganese has become an inevitable trend in the development of the industry.In this study,using electrolytic manganese as raw material,through self-developed high-efficiency distillation furnace,the high-purity manganese with a purity of more than 4N5 was prepared in one step combined with partition condensation,the length of the main metal condensation zone was extended by setting a constant temperature condensation section in the condensation zone to achieve the purpose of improving the metal yield.The theory of vacuum distillation of electrolytic manganese was analyzed,and the effects of different distillation temperatures and times on the volatilization rate and the temperature of the constant temperature condensation section(condensation temperature)on the metal yield were studied.At the same time,the impurity content in the condensed manganese at different distillation temperatures was detected by inductively coupled plasma mass spectrometry(ICP-MS).The results show that the main metal Mn is easy to separate from the impurity metal at the selected distillation temperature,but the higher the temperature,the weaker the separation ability.With the increase of distillation temperature and holding time,the volatilization rate increases.Setting the main metal constant temperature condensation section can greatly improve the me-tal yield,with the increase of condensation temperature,the metal yield increases first and then decreases.With the increase of distillation temperature,the contents of Cd,K,Na,and Zn in condensed manganese are almost unchanged,while the contents of Mg,Ca,Pb,Cu,Cr,Ni,Fe,and Co increased with the increase of distillation temperature.Considering comprehensively,high-purity manganese with the purity of 4N5 can be obtained under a system pressure of 10^(-3)—10^(-2)Pa,a condensation temperature of 1100℃,a holding time of 90 min,and a distillation temperature of 1400℃.In this instance,the volatilization rate is 86.94%,and the yield can reach 94.32%.
作者
孙院军
赵永喆
杨双平
丁向东
孙军
SUN Yuanjun;ZHAO Yongzhe;YANG Shuangping;DING Xiangdong;SUN Jun(College of Materials Science and Engineering,Xi’an Jiaotong University,Xi’an 710049,China;College of Metallurgical Engineering,Xi’an University of Architecture and Technology,Xi’an 710055,China)
出处
《材料导报》
北大核心
2025年第12期104-108,共5页
Materials Reports
基金
陕西省重点研发计划项目(2020ZDZX04-02-01HZ)。
关键词
高纯锰
真空蒸馏
电解锰
一步法
分区冷凝
high purity manganese
vacuum distillation
electrolytic manganese
one-step method
partition condensation
作者简介
孙院军,博士,西安交通大学材料科学与工程学院教授、博士研究生导师。目前主要从事钼合金、难熔合金方面的研究工作。;通信作者:杨双平,博士,西安建筑科技大学冶金工程学院教授、博士研究生导师。目前主要从事炼铁方面的研究工作。yang_sping@163.com。
